HRID1616337

反应详情

EQUATION

反应方程式

HRID 1616337 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
0 °C

PROCEDURE

实验过程

To a solution of 2-amino-5-bromobenzoic acid (50 g) in water (200 mL) was added HCl (46 mL). To the mixture was added aqueous NaNO2 solution (17.7 g/37 mL) at 0° C., and the mixture was stirred at 0° C. for 30 minutes. To the reaction solution was added dropwise aqueous Na2SO3 solution (79.3 g/200 mL) at 0° C., and the mixture was stirred at room temperature for 2 hours. To the mixture was added HCl (70 mL), and the mixture was stirred at room temperature for 18 hours and then at 80° C. for 4 hours. The precipitated solid was dissolved by basifying the reaction solution, and then the solution was acidified to precipitate a solid. The solid was collected by filtration and dried under reduced pressure to give Compound Q2 (36 g).

WORKUP

后处理

  1. stirringthe mixture was stirred at room temperature for 2 hours
  2. stirringthe mixture was stirred at room temperature for 18 hours
  3. waitat 80° C. for 4 hours
  4. dissolutionThe precipitated solid was dissolved
  5. customto precipitate a solid
  6. filtrationThe solid was collected by filtration
  7. customdried under reduced pressure
  8. customto give Compound Q2 (36 g)